NDLI: Ultrasonic-assisted derivatization of estrogenic compounds in a cup horn booster and determination by GC-MS.

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Ultrasonic-assisted derivatization of estrogenic compounds in a cup horn booster and determination by GC-MS.

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Ultrasonic-assisted derivatization of estrogenic compounds in a cup horn booster and determination by GC-MS.

Content Provider	World Health Organization (WHO)-Global Index Medicus
Author	Vallejo, Asier Usobiaga, Aresatz Martinez-Arkarazo, Irantzu Prieto, Ailette Etxebarria, Nestor Zuloaga, Olatz Fernández, Luis A.
Description	Country affiliation: Spain Author Affiliation: Vallejo A ( Department of Analytical Chemistry, University of Basque Country, Bilbao, Spain. asier.vallejo@ehu.es)
Abstract	Cup horn boosters are miniaturized ultrasound baths that maximize efficiency and precision. The optimization of an ultrasonic-assisted derivatization step by means of a cup horn booster and the determination of estrone, 17beta-estradiol, estriol, 17alpha-ethynyl estradiol and mestranol was developed by GC-MS. Different derivatization reagents and solvents were studied for maximizing the di-derivatization of 17alpha-ethynyl estradiol under ultrasound energy. Only N,O-bis(trimethylsilyl)trifluoroacetamide with 1% of trimethylchlorosilane in pyridine gave satisfactory results and this mixture was further used in the optimization of the ultrasound assisted derivatization. The experiment designs included sonication time (1-10 min), sonication power (20-80%), sonication cycles (1-9), derivatization reagent volume (25-125 microL) and solvent volume (25-125 microL). Once the optimum conditions were fixed, the effect of organic matter and the frequency of the water bath change were studied. Finally, the validation of the analytical method was carried out using spiked natural and synthetic waters. Recoveries (natural (138-70%) and synthetic (112-89%)), the LODs (0.35-1.66 ng/L), and LOQs (1.16-5.52 ng/L) and the precision (0.2-5.3%) of the method were studied. This is the first work in the literature where a cup horn booster is used with the aim of minimizing derivatization time during the determination of estrogenic compounds.
File Format	HTM / HTML
ISSN	16159306
Issue Number	1
Volume Number	33
e-ISSN	16159314
Journal	Journal of Separation Science
Language	English
Publisher	Wiley-VCH
Publisher Date	2010-01-01
Publisher Place	Germany
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	Discipline Analytical Discipline Chemistry Estrogens Analysis Gas Chromatography-mass Spectrometry Ultrasonics Acetamides Chemistry Animals Estradiol Estriol Estrone Ethinyl Estradiol Female Instrumentation Methods Humans Indicators And Reagents Male Mestranol Solvents Trimethylsilyl Compounds Water Pollutants, Chemical Journal Article Research Support, Non-u.s. Gov't
Content Type	Text
Resource Type	Article
Subject	Analytical Chemistry Filtration and Separation

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